Cyclic utilization method of production mother liquor of 4-ethyl-2, 3-dioxopiperazine-1-formyl chloride

A technology of dioxypiperazine and formyl chloride, applied in the field of pharmaceutical intermediate 4-ethyl-2,3-dioxypiperazine-1-formyl chloride, which can solve the problem of harmless treatment and lack of high added value , high cost and other issues, to achieve the effect of comprehensive utilization of high added value, green and economical production process, and easy operation

Pending Publication Date: 2020-08-07
山西新天源药业有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] Although the above-mentioned traditional treatment process for producing mother liquor is relatively simple and mature, there are mainly three deficiencies in the following aspects: 1) The residual trimethylchlorosilane and target products in the production mother liquor are directly hydrolyzed and destroyed, and cannot be processed with high added value. Utilization; 2) After the production mother liquor is destroyed by adding alkaline water, it not only needs to consume a large amount of alkali liquor, but also produces a large amount (about ...

Method used

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  • Cyclic utilization method of production mother liquor of 4-ethyl-2, 3-dioxopiperazine-1-formyl chloride
  • Cyclic utilization method of production mother liquor of 4-ethyl-2, 3-dioxopiperazine-1-formyl chloride
  • Cyclic utilization method of production mother liquor of 4-ethyl-2, 3-dioxopiperazine-1-formyl chloride

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Effect test

Embodiment 1

[0026] CN 101417982A embodiment 1 uses dichloromethane as reaction solvent, raw material 4-ethyl-2,3-dioxypiperazine, trimethylchlorosilane, triethylamine and bis-(trichloromethyl)carbonate are reacted , After removing insoluble matter from the reaction solution, dipropyl ether is added dropwise to precipitate white needle crystals of 4-ethyl-2,3-dioxypiperazine-1-formyl chloride and produce a mother liquor. The IR spectrum of the target product of 4-ethyl-2,3-dioxypiperazine-1-formyl chloride is shown in figure 1 .

[0027] In this embodiment, 1400 kg of the above-mentioned production mother liquor is added to a 2000L reflux kettle, stirring is started, the corresponding valve of the reflux system is opened, and the three-stage lye falling film absorption device and the first-stage activated carbon adsorption device of the emptying system are opened to raise the temperature of the production mother liquor To the reflux temperature, timer reflux for 60min.

[0028] After the...

Embodiment 2

[0035] CN 101417982A embodiment 2 uses chloroform as the reaction solvent, and the raw materials 4-ethyl-2,3-dioxypiperazine, trimethylchlorosilane, triethylamine and bis-(trichloromethyl) carbonate are reacted, and the reaction After removing the insoluble matter, the crystallization agent n-hexane was added dropwise to precipitate white needle crystals of 4-ethyl-2,3-dioxypiperazine-1-formyl chloride and produce the production mother liquor.

[0036] In this embodiment, 620 g of the above-mentioned production mother liquor is added to a 1000 ml three-necked reaction flask equipped with a thermometer, mechanical stirring and a reflux condenser, and the stirring is started, and the exhaust port of the reflux condenser is connected to a buffer bottle and a three-stage lye washing machine through an air duct. Cylinders, raise the temperature of the production mother liquor to the reflux temperature, and time the reflux for 120 minutes.

[0037] After the reflux, monitor that the...

Embodiment 3

[0043] CN 101417982A embodiment 3 uses dichloromethane as the reaction solvent, and the raw materials 4-ethyl-2,3-dioxypiperazine, trimethylchlorosilane, triethylamine and bis-(trichloromethyl) carbonate are reacted , After removing insoluble matter from the reaction solution, the crystallization agent petroleum ether is added dropwise to precipitate white needle crystals of 4-ethyl-2,3-dioxypiperazine-1-formyl chloride and produce a production mother liquor.

[0044] In this embodiment, 580 g of the above-mentioned production mother liquor is added to a 1000 ml three-necked reaction flask equipped with a thermometer, mechanical stirring and a reflux condenser, and the stirring is started, and the exhaust port of the reflux condenser is connected to a buffer bottle and a three-stage lye washing machine through an air duct. Cylinder, raise the temperature of the production mother liquor to the reflux temperature, and time the reflux for 20 minutes.

[0045] After the reflux is ...

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Abstract

The invention discloses a cyclic utilization method of production mother liquor in a production method of 4-ethyl-2, 3-dioxopiperazine-1-formyl chloride in CN10147982A. The method comprises the stepsof: carrying out heating reflux treatment on production mother liquor to decompose a small amount of residual bis (trichloromethyl) carbonate, carrying out distillation separation treatment to obtaina distillate and a residual solution, recycling the distillate in the production process of 4-ethyl-2, 3-dioxopiperazine-1-formyl chloride, and recycling the residual solution in the crystallization process of 4-ethyl-2, 3-dioxopiperazine-1-formyl chloride. According to the cyclic utilization method, high-added-value comprehensive utilization of all effective components in the production mother liquor is achieved, production and product performance of 4-ethyl-2, 3-dioxopiperazine-1-formyl chloride cannot be affected, the yield of the target product can be increased to 88.0% or above, and the purity can reach 97.0% or above.

Description

technical field [0001] The present invention relates to the production technology of pharmaceutical intermediate 4-ethyl-2,3-dioxopiperazine-1-formyl chloride, in particular to a kind of 4-ethyl-2,3-dioxypiperazine-1-formyl chloride A method for recycling the production mother liquor produced in the production of acid chlorides. Background technique [0002] CN 101417982A discloses a synthesis and crystallization method of 4-ethyl-2,3-dioxypiperazine-1-formyl chloride, which uses 4-ethyl-2,3-dioxypiperazine as a starting material, Trimethylchlorosilane ((CH 3 ) 3 SiCl) is the activator and protective agent, triethylamine is the acid-binding agent and catalyst, reacts with the formyl chloride reagent bis(trichloromethyl)carbonate (BTC) in the reaction solvent, and filters out the insoluble triethylamine salt , adding a crystallization agent to obtain crystallization of the target product 4-ethyl-2,3-dioxypiperazine-1-formyl chloride. The specific reaction equation is as f...

Claims

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Application Information

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IPC IPC(8): C07D241/08
CPCC07D241/08
Inventor 苏蔚汤芝平陈万成苏斌林高志伟康福堂
Owner 山西新天源药业有限公司
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